应用化学 ›› 1997, Vol. 0 ›› Issue (6): 66-68.

• 研究论文 • 上一篇    下一篇

用高效液相色谱法优化苯与对氯氯苄烷基化反应催化剂

刘红霞1, 张书胜1, 袁倬斌2   

  1. 1. 郑州大学分析测试中心, 郑州;
    2. 中国科学技术大学研究生院, 北京 100039
  • 收稿日期:1997-03-31 修回日期:1997-09-05 出版日期:1997-12-10 发布日期:1997-12-10
  • 基金资助:
    国家自然科学基金;河南省分析测试基金

Optimization of Catalyst for the Alkylation Reaction of Benzene and p-Chlorobenzyl Chloride by HighPerformance Liquid Chromatography

Liu Hongxia1, Zhang Shusheng1, Yuan Zhuobin2   

  1. 1. Center of Analysis and Test, Zhengzhou University, Zhengzhou;
    2. Graduate School, University of Science and Technology of China, Chinese Academy of Sciences, Beijing 100039
  • Received:1997-03-31 Revised:1997-09-05 Published:1997-12-10 Online:1997-12-10

摘要: 对氯-二苯甲烷(p-CDPM)是许多药物的重要中间体[1], 可由苯与对氯氯苄烷基化反应制取. 在合成P-CDPM的过程中, 会有异构体m-CDPM与o-CDP M生成[2~4]. 在提高P-CDPM和降低 o, m-CDPM 的产率研究中, 建立快速测定 o, m, P-CDPM 的定量分析方法具有重要意义。

关键词: 氯-二苯甲烷, 制备, 三氯化铝, 硝基苯, 硝基乙烷, 高效液相色谱法

Abstract: The high-performance liquid chromatography(HPLC)has been used for quantitative determination of o,m,P-chlorodiphenylmethane(CDPM)from the reaction products of benzene with P-chlorobenzyl chloride for P-CDPM preparation. The detection limits of the method for o,m,P-CDPM were 0.35, 0.40 and 0.32 mg/L, respectively. The method was applied to gain the optimum constitution of the catalysts used in the preparation. The results showed that nitro compounds could prevent the decomposition of diphenylmethane and its chloride. The yield of PCDPM was higher than 96%, when AlCl3(4g)+EtNO2(1.5 mL)were used as catalyst.

Key words: chlorodiphenylmethane, preparation, aluminium trichloride, nitrobenzene, nitroethane, HPLC